CN107902681A - A kind of preparation method of calcium aluminum hydrotalcite - Google Patents
A kind of preparation method of calcium aluminum hydrotalcite Download PDFInfo
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- CN107902681A CN107902681A CN201711233019.0A CN201711233019A CN107902681A CN 107902681 A CN107902681 A CN 107902681A CN 201711233019 A CN201711233019 A CN 201711233019A CN 107902681 A CN107902681 A CN 107902681A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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Abstract
The invention discloses a kind of preparation method of calcium aluminum hydrotalcite, and calcium hydroxide, aluminium hydroxide and sodium carbonate are added in ball mill, and ball material mass ratio is controlled 8~12：1, rotational speed of ball-mill is 200~500r/min, dry grind 2~4h, it is small, in, big abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio be 1~2：2~3：5~7；Solid mixture is mixed with water, under 600~800W, at 70~90 DEG C, 5~20min of microwave hydrothermal crystallization；Washing, filtering, drying, obtain calcium aluminum hydrotalcite." one kettle way dry grinding " is combined by this method with " microwave hydrothermal crystallization ", is simplified calcium aluminum hydrotalcite preparation flow, is shortened preparation time, simplifies operation, improves efficiency, and product structure is more single.Compared to existing calcium aluminum hydrotalcite preparation method, present invention process flow is simple, it is time-consuming it is short, easy to operate, yield is high, product is single.
Description
Technical field
The present invention relates to hydrotalcite synthesis technical field, and in particular to a kind of preparation method of calcium aluminum hydrotalcite.
Background technology
Hydrotalcite material belongs to anion type laminated compound.Lamellar compound refers to layer structure, interlayer ion,
A kind of compound with interchangeability, using lamellar compound main body under highly polar molecular action possessed by intercalation
With the interchangeability of interlayer ion, some feature guest species are introduced into bedding void and are strutted laminate distance so as to be formed
Layer-pillared compound.Hydrotalcite-based compound (LDHs) is a kind of novel inorganic functional material with layer structure, the master of LDHs
Body laminate chemical composition and its laminate cationic characteristic, laminate charge density or anion exchange capacity, supermolecular intercalation structure
It is closely related etc. factor.
In general, as long as metal cation has suitable ionic radius (with Mg2+Ionic radius 0.072nm difference
Less) and charge number, LDHs laminates can be formed.LDHs be passed through by positively charged main layer board and interlayer anion it is non-common
The compound that the interaction assembling of valence link forms, its structure are similar to shepardite Mg (OH)2, by MgO6The shared rib of octahedron
Form elementary layer.There is the characteristics of following very prominent：(1) chemical composition of main layer board can modulation；(2) interlayer object the moon from
The type and quantity of son can modulation；(3) grain size of intercalation assembly and distribution are controllable.The design feature of LDHs makes its layer
Between anion can be with various anion, including inorganic ions, organic ion, ion of the same race, heteropoly acid ion and ligand compound
The anion of thing swaps.It can be synthesized using this property of LDHs with the species of modulation interlayer anion different types of
LDHs, and its different property is assigned, so as to obtain the new material with difference in functionality.At present, its application is mainly as hot steady
Determine agent, fire retardant, adsorbent, catalyst, construction material, pharmaceutical carrier etc..
LDHs preparation methods have coprecipitation, structural remodeling method, salt-conventional ceramic technique, induced hydrolysis method, sol-gel process,
Hydrothermal synthesis method, nucleation/crystallization isolation method etc..These methods are uneven there are particle diameter distribution, or crystalline form is bad, or complex process,
Or cost is excessive, or the shortcomings of unsuitable large-scale production.
CN105802070A patents are using powder calcium hydroxide and aluminium hydroxide as raw material, using deionized water as solvent, room
The rotating speed stirring 0.5h of 800~1000r/min of temperature, then add natrium carbonicum calcinatum, continue to stir 0.5h, then under 60~75 DEG C of oil baths
15~25h of stirring reaction under same rotational speed, then be washed with deionized, it is dry, obtain calcium aluminum hydrotalcite, structural formula Ca4Al2
(OH)12CO3·5H2O.For the patent using water as reaction dissolvent, selection uses natrium carbonicum calcinatum, and calcium in obtained hydrotalcite
Al atomic ratio is 2:1, cost is higher；In addition, whole preparation process needs more than 16h, the time is partially long；Also, calcium hydroxide and
Aluminium hydroxide feeds intake with natrium carbonicum calcinatum in a manner of in batches, and operation is more troublesome.
CN105271343A patents are using calcium hydroxide and aluminium hydroxide as raw material, and elder generation is dry grinded successively, wet-milling is some small
When, sodium carbonate liquor water-bath crystallization is added, centrifuge washing is dry to obtain hydrocalumite, structural formula Ca16Al8(OH)54CO3·2H2O.The patent Ball-milling Time is longer (5~8h), and calcium al atomic ratio is 2 in hydrocalumite:1, cost is higher；And hydrogen
Calcium oxide and aluminium hydroxide are also to feed intake in a manner of in batches with sodium carbonate, equally exist the problem of troublesome in poeration.
The content of the invention
It is an object of the present invention to overcome the shortcomings of to mention in background above technology and defect, there is provided a kind of technological process
Simply, the preparation method of the calcium aluminum hydrotalcite short, easy to operate, yield is high, product structure is single is taken.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of preparation method of calcium aluminum hydrotalcite, comprises the following steps：Calcium hydroxide, aluminium hydroxide and sodium carbonate are added
In ball mill, ball material mass ratio is controlled in (8~12)：1, rotational speed of ball-mill is 200~500r/min, and dry grind 2~4h, obtains solid and mixes
Compound, abrading-ball used in mechanical milling process be divided into it is small, in, big three kinds of specifications, it is small, in, the diameter of big abrading-ball be respectively 5mm, 8mm and
10mm, it is small, in, the quantity ratio of big abrading-ball be (1~2)：(2~3)：(5~7)；Obtained solid mixture is mixed to form with water
Solidliquid mixture, then solidliquid mixture is subjected to microwave hydrothermal crystallization, microwave power control is in 600~800W, crystallization temperature
70~90 DEG C, crystallization time is 5~20min；Then in turn through filter, washing, drying, up to calcium aluminum hydrotalcite.
The present invention is creatively by three kinds of calcium hydroxide, aluminium hydroxide and sodium carbonate components by " one kettle way " in ball mill
Middle dry grinding, the diameter and ratio of control ball material mass ratio and large, medium and small abrading-ball in mechanical milling process, then by microwave hydrothermal
Crystallization, obtains target product.Inventor is had found by lot of experiments, under the conditions of having existing for water, three kinds of component raw materials
Using " one kettle way " under ball milling or high-speed stirred, preferable product cannot be obtained, this is because calcium hydroxide is slightly soluble in water,
Sodium carbonate easily forms the precipitation of calcium carbonate for being insoluble in water with the calcium hydroxide that is dissolved in water, can take in final product and
It can not separate.And under the conditions of dry grinding, Ca2+、Al3+As central ion, CO3 2-、OH-As coordination ion, OH-Half
Footpath is small, electrically charged few, CO3 2-Radius is big, and institute is electrically charged more, therefore OH-Coordination ability it is strong, therefore, OH-Preferentially and Ca2+、Al3+
It is coordinated and forms hydrotalcite veneer structure, and CO3 2-In interlayer and the unnecessary positive charge of laminate, formation can between regulating layer the moon from
Son." one kettle way " synthesis of calcium aluminum hydrotalcite is realized, three kinds of raw materials need to be only added in ball mill together, control ball abrasive stick
Part, dry grind 2~4h, then carries out microwave hydrothermal crystallization.Be conducive to improve the crystalline phase pattern of product using microwave hydrothermal crystallization,
And it can further shorten the reaction time.
The present invention passes through " one kettle way dry grinding " and " Microwave Water using the method for " one kettle way dry grinding "+" microwave hydrothermal crystallization "
Collaboration between two steps of thermal crystallisation ", while control ball material mass ratio, rotational speed of ball-mill, abrading-ball in " one kettle way dry grinding " step
Specification and ratio, control " microwave hydrothermal crystallization " microwave power, crystallization temperature and time so that prepared product structure
Single, yield is high, and substantially reduces the reaction time.Compared to the preparation method of existing calcium aluminum hydrotalcite, the present invention has
Technological process is simple, time-consuming short, easy to operate, yield high (yield up to more than 90%), the advantages that product structure is single, be suitable for
Industrialization large-scale production.
As preferable scheme, it is described it is small, in, the quantity ratio of big abrading-ball be 1：3：6.It is more advantageous to obtaining under the ratio
The single product of structure.
As preferable scheme, the rotating speed of ball mill is 220~250r/min in the dry milled process.
As preferable scheme, the microwave hydrothermal crystallization steps are specially：It is anti-that solidliquid mixture is placed in microwave hydrothermal
Answer in kettle, microwave power control is controlled at 75~85 DEG C in 700~750W, crystallization temperature, and crystallization time is 5~10min.
As preferable scheme, the granularity of the calcium hydroxide, aluminium hydroxide and sodium carbonate is all higher than 200 mesh.
As preferable scheme, the addition of the water is 1~3 times of solid mixture quality.
As preferable scheme, the water-washing step specifically refers to：With tap water or deionized water by the product after crystallization
Wash to neutrality.
As preferable scheme, byproduct hydrogen is obtained after waste water that the water-washing step and filtration step are obtained is concentrated
Sodium oxide molybdena.
As preferable scheme, the molar ratio of the calcium hydroxide, aluminium hydroxide and sodium carbonate is 8：2：(1~4),
The molecular formula of the calcium aluminum hydrotalcite is Ca8Al2(OH)20CO3·6H2O。
Calcium aluminum hydrotalcite product with new structure can be prepared by the special preparation method of the present invention
(Ca8Al2(OH)20CO3·6H2O), the atomic ratio of calcium and aluminium brings up to 4 in the calcium aluminum hydrotalcite：1 (existing calcium aluminum hydrotalcite calcium
Al atomic ratio is mostly 3：1 or less), effectively reduce the cost of raw material (aluminium hydroxide is more expensive than calcium hydroxide).Also, according to meter
Calculate, since calcium ion radius ratio aluminium ion radius is much bigger, calcium aluminium ratio increases to 4：1, can reach hydrotalcite layer distance between plates
To maximum so that between laminate can anion can be preferably by the more anion exchanges of species, so as to obtain between regulating layer
Follow-up widely application.
Compared with prior art, the advantage of the invention is that：
(1) preparation method of the invention, in terms of synthesis, by the reaction of aluminium hydroxide and calcium hydroxide, aluminium hydroxide and
Anion exchange reaction between the reaction product and sodium carbonate of calcium hydroxide, has been dry grinded in the ball mill by " one kettle way "
Into, be effectively simplified the preparation flow of calcium aluminum hydrotalcite, shorten preparation time, simplify operation, improve production effect
Rate.
(2) preparation method of the invention, passes through the association between " one kettle way dry grinding " and " microwave hydrothermal crystallization " two steps
Together, by controlling the specification and ratio of ball material mass ratio, abrading-ball in " one kettle way dry grinding " step, control " microwave hydrothermal crystallization "
Microwave power, crystallization temperature and time so that prepared product structure is single, and yield is high, and substantially reduces the reaction time.
(3) can obtain molecular formula by the preparation method of the present invention is Ca8Al2(OH)20CO3·6H2The new structure of O
Calcium aluminum hydrotalcite, the atomic ratio of calcium aluminium is 4 in the calcium aluminum hydrotalcite：1, it is mostly 3 compared to existing calcium al atomic ratio：1 and with
Under calcium aluminum hydrotalcite product, products obtained therefrom cost of the present invention is lower, and neatly stone veneer spacing in the calcium aluminum hydrotalcite structure
From bigger, between laminate can anion can be preferably wider by the more anion exchanges of species, application range between regulating layer.
(4) by the present invention preparation method can be in high yield obtain the calcium aluminum hydrotalcite product of new structure, its yield
Up to more than 90%；The preparation method of present invention water used in preparation process can be tap water or deionized water, with originally
Water can also equally obtain target product in high yield as water source, reduce further manufacturing cost.
To sum up, the preparation method of the present invention have technological process it is simple, it is time-consuming it is short, easy to operate, cost is low, yield
High, the advantages that product structure is single, it is suitable for industrialization large-scale production；And it can obtain in high yield with new structure
Ca8Al2(OH)20CO3·6H2O calcium aluminum hydrotalcite products, the calcium al atomic ratio of the calcium aluminum hydrotalcite product is high, compared to existing
Calcium aluminum hydrotalcite product, resulting product application range of the present invention are wider.
Brief description of the drawings
Fig. 1 is the process flow chart of calcium aluminum hydrotalcite preparation method of the present invention.
Fig. 2 is the XRD spectra of 1 gained calcium aluminum hydrotalcite of the embodiment of the present invention.
Fig. 3 is the IR spectrograms of 1 gained calcium aluminum hydrotalcite of the embodiment of the present invention.
Fig. 4 is that the TG/DSC of 1 gained calcium aluminum hydrotalcite of the embodiment of the present invention schemes.
Embodiment
For the ease of understanding the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood implication of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
Weigh respectively powdered calcium hydroxide 59.3g (0.8mol, more than 200 mesh), aluminium hydroxide 15.6g (0.2mol, greatly
In 200 mesh), solid sodium carbonate 10.6g (0.1mol, more than 200 mesh) sequentially add in ball grinder, ball milling 2h, rotational speed of ball-mill is
220r/min, it is small, in, big abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio be 1：3：6, solid mixture is obtained, then will
Solid mixture is transferred in microwave hydrothermal reaction kettle, adds deionized water 170g, at microwave power 700W, 85 DEG C, crystallization
5min, is then centrifuged for filtering, and is washed with deionized to neutrality, forced air drying at 80 DEG C, crush, weigh to obtain molecular formula be
Ca8Al2(OH)20CO3·6H2The calcium aluminum hydrotalcite product 80.5g of O, yield 91.3%.
The XRD spectra of gained calcium aluminum hydrotalcite product as shown in Fig. 2, from Figure 2 it can be seen that 2 θ be 11.7 °, 23.4 °, 35.6 °,
38.5 °, 46.7 °, the characteristic diffraction peak that 61.2 ° etc. diffraction maximums are hydrotalcite-based compound, product structure are single.Gained calcium aluminium
The IR spectrograms of hydrotalcite product are as shown in figure 3, as seen from Figure 3,3500~3600cm-1Place's broad peak is OH-Characteristic absorption peak, shows
There is hydroxyl generation in product；1420cm-1Place is CO3 2-Characteristic absorption peak, shows there is carbonate generation in product；400~
800cm-1Place is the characteristic absorption peak band of Ca-O and Al-O keys.Gained calcium aluminum hydrotalcite product TG/DSC figure as shown in figure 4, by
Fig. 4 as it can be seen that before 200 DEG C weightlessness 12.63%, this be discharge laminate between with reference to hydrone caused by, pass through calculating, it can be deduced that
Product molecule contains 6 crystallizations water.Product elemental analysis result shows that its calcium aluminium ratio is 4：1.
Embodiment 2：
Weigh respectively powdered calcium hydroxide 59.3g (0.8mol, more than 200 mesh), aluminium hydroxide 15.6g (0.2mol, greatly
In 200 mesh), solid sodium carbonate 10.6g (0.1mol, more than 200 mesh) sequentially add in ball grinder, ball milling 3h, rotational speed of ball-mill is
220r/min, it is small, in, big abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio be 1：3：6, solid mixture is obtained, then will
Solid mixture adds deionized water 170g into microwave hydrothermal reaction kettle, at microwave power 700W, 85 DEG C, crystallization 5min,
It is then centrifuged for filtering, is washed with deionized to neutrality, forced air drying at 80 DEG C, crushes, it is Ca to weigh to obtain molecular formula8Al2
(OH)20CO3·6H2The calcium aluminum hydrotalcite product 81.0g of O, yield 91.8%.
Embodiment 3：
Weigh respectively powdered calcium hydroxide 59.3g (0.8mol, more than 200 mesh), aluminium hydroxide 15.6g (0.2mol, greatly
In 200 mesh), solid sodium carbonate 10.6g (0.1mol, more than 200 mesh) sequentially add in ball grinder, ball milling 4h, rotational speed of ball-mill is
220r/min, it is small, in, big abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio be 1：3：6, solid mixture is obtained, then will
Solid mixture is transferred in microwave hydrothermal reaction kettle, adds deionized water 170g, at microwave power 700W, 85 DEG C, crystallization
5min, is then centrifuged for filtering, and with originally water washing to neutrality, forced air drying at 80 DEG C, crushes, weigh to obtain molecular formula be
Ca8Al2(OH)20CO3·6H2The calcium aluminum hydrotalcite product 81.2g of O, yield 92.1%.
Embodiment 4：
Weigh respectively powdered calcium hydroxide 59.3g (0.8mol, more than 200 mesh), aluminium hydroxide 15.6g (0.2mol, greatly
In 200 mesh), solid sodium carbonate 10.6g (0.1mol, more than 200 mesh) sequentially add in ball grinder, ball milling 3h, rotational speed of ball-mill is
220r/min, it is small, in, big abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio be 1：3：6, solid mixture is obtained, then will
Solid mixture is transferred in microwave hydrothermal reaction kettle, adds deionized water 170g, at microwave power 700W, 85 DEG C, crystallization
5min, is then centrifuged for filtering, and with originally water washing to neutrality, forced air drying at 80 DEG C, crushes, weigh to obtain molecular formula be
Ca8Al2(OH)20CO3·6H2The calcium aluminum hydrotalcite product 81.0g of O, yield 91.8%.
Embodiment 5：
Weigh respectively powdered calcium hydroxide 59.3g (0.8mol, more than 200 mesh), aluminium hydroxide 15.6g (0.2mol, greatly
In 200 mesh), solid sodium carbonate 21.2g (0.2mol, more than 200 mesh) sequentially add in ball grinder, ball milling 3h, rotational speed of ball-mill is
220r/min, it is small, in, big abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio be 1：3：6, solid mixture is obtained, then will
Solid mixture is transferred in microwave hydrothermal reaction kettle, adds deionized water 170g, at microwave power 700W, 85 DEG C, crystallization
5min, is then centrifuged for filtering, and with originally water washing to neutrality, forced air drying at 80 DEG C, crushes, weigh to obtain molecular formula be
Ca8Al2(OH)20CO3·6H2The calcium aluminum hydrotalcite product 79.8g of O, yield 90.5%.
Comparative example 1：
It is 8 by the amount of material：2：1~4 ratio weighs calcium hydroxide, aluminium hydroxide and sodium carbonate and (is all higher than 200 respectively
Mesh), calcium hydroxide and aluminium hydroxide are placed in ball grinder by load weighted sodium carbonate wiring solution-forming, adjusting rotational speed of ball-mill is
250r/min, it is small, in, big abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio be 1：3：6,6h is ground, is then added excessive
Deionized water continues to grind 2h.Obtained material is taken out and is put into flask, the sodium carbonate liquor being configured is added, 80
Insulation reaction 4h under DEG C water-bath.Flask is down to room temperature after reaction, removes supernatant liquor, the production that will be obtained with deionized water
Product are rinsed to neutrality and filtered, and filter cake is placed in drying in 80 DEG C of vacuum drying chamber, obtains product, its X- diffracting spectrum is shown
There is obvious CaCO3Characteristic diffraction peak, product are mixture, can not obtain structure single product.
Comparative example 2：
Powdered calcium hydroxide 59.3g (0.8mol), aluminium hydroxide 15.6g (0.2mol), solid sodium carbonate are weighed respectively
10.6g (0.1mol) is sequentially added in ball grinder and (is all higher than 200 mesh), ball milling 2h, rotational speed of ball-mill 220r/min, it is small, in, it is big
Abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio is 6：3：1, solid mixture is obtained, is then transferred to solid mixture micro-
In ripple hydrothermal reaction kettle, deionized water 170g is added, at microwave power 700W, 85 DEG C, crystallization 5min, is then centrifuged for filtering,
It is washed with deionized to neutrality, forced air drying at 80 DEG C, crushes, obtained product X-diffracting spectrum is shown significantly
CaCO3Characteristic diffraction peak and aluminium hydroxide characteristic diffraction peak, product are mixture, can not obtain structure single product.
Comparative example 3：
Powdered calcium hydroxide 59.3g (0.8mol), aluminium hydroxide 15.6g (0.2mol), solid sodium carbonate are weighed respectively
10.6g (0.1mol) is sequentially added in ball grinder and (is all higher than 200 mesh), ball milling 2h, rotational speed of ball-mill 220r/min, it is small, in, it is big
Abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio is 3：6：1, solid mixture is obtained, is then transferred to solid mixture micro-
In ripple hydrothermal reaction kettle, deionized water 170g is added, at microwave power 700W, 85 DEG C, crystallization 5min, is then centrifuged for filtering,
It is washed with deionized to neutrality, forced air drying at 80 DEG C, crushes, obtained product X-diffracting spectrum is shown significantly
CaCO3Characteristic diffraction peak and aluminium hydroxide characteristic diffraction peak, it is mixture to show product, can not obtain structure single product.
Comparative example 4：
Powdered calcium hydroxide 59.3g (0.8mol), aluminium hydroxide 15.6g (0.2mol), solid sodium carbonate are weighed respectively
10.6g (0.1mol) is sequentially added in ball grinder and (is all higher than 200 mesh), ball milling 2h, rotational speed of ball-mill 220r/min, it is small, in, it is big
Abrading-ball (diameter is respectively 5mm, 8mm, 10mm) ratio is 1：3：6, solid mixture is obtained, solid mixture is then transferred to burning
In cup, deionized water 170g is added, water-bath insulation crystallization 5min at 85 DEG C, is then centrifuged for filtering, is washed with deionized into
Property, forced air drying at 80 DEG C crushes, and obtains product X-diffracting spectrum characteristic diffraction peak unobvious.
Claims (8)
1. a kind of preparation method of calcium aluminum hydrotalcite, it is characterised in that comprise the following steps：By calcium hydroxide, aluminium hydroxide and
Sodium carbonate is added in ball mill, and ball material mass ratio is controlled in (8~12)：1, rotational speed of ball-mill is 200~500r/min, dry grinding 2~
4h, obtains solid mixture, abrading-ball used in mechanical milling process be divided into it is small, in, big three kinds of specifications, it is small, in, the diameter of big abrading-ball be respectively
5mm, 8mm and 10mm, it is small, in, the quantity ratio of big abrading-ball be (1~2)：(2~3)：(5~7)；By obtained solid mixture and water
Solidliquid mixture is mixed to form, then solidliquid mixture is subjected to microwave hydrothermal crystallization, microwave power control is in 600~800W, crystalline substance
It is 70~90 DEG C to change temperature, and crystallization time is 5~20min；Then in turn through filter, washing, drying, up to calcium aluminum hydrotalcite.
2. the preparation method of calcium aluminum hydrotalcite according to claim 1, it is characterised in that ball mill in the dry milled process
Rotating speed be 220~250r/min.
3. the preparation method of calcium aluminum hydrotalcite according to claim 1, it is characterised in that the microwave hydrothermal crystallization steps
Specially：Solidliquid mixture is placed in microwave hydrothermal reaction kettle, microwave power is controlled in 700~750W, crystallization temperature 75
~85 DEG C, crystallization time is 5~10min.
4. the preparation method of calcium aluminum hydrotalcite according to claim 1, it is characterised in that calcium hydroxide, aluminium hydroxide and
The granularity of sodium carbonate is all higher than 200 mesh.
5. the preparation method of calcium aluminum hydrotalcite according to claim 1, it is characterised in that the addition of the water is solid
1~3 times of mixture quality.
6. the preparation method of calcium aluminum hydrotalcite according to claim 1, it is characterised in that the water-washing step is specifically
Refer to：The product after crystallization is washed to neutrality with tap water or deionized water.
7. the preparation method of calcium aluminum hydrotalcite according to claim 1, it is characterised in that by the water-washing step and filtering
Byproduct sodium hydroxide is obtained after waste water that step obtains is concentrated.
8. according to the preparation method of calcium aluminum hydrotalcite according to any one of claims 1 to 7, it is characterised in that the hydrogen-oxygen
The molar ratio for changing calcium, aluminium hydroxide and sodium carbonate is 8：2：(1~4), the molecular formula of the calcium aluminum hydrotalcite is Ca8Al2
(OH)20CO3·6H2O。
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| CN109437291A (en) * | 2018-12-24 | 2019-03-08 | 中南民族大学 | Hydrotalcite and preparation method thereof |
| CN109939683A (en) * | 2019-04-09 | 2019-06-28 | 江苏新沃催化剂有限公司 | A kind of ternary compound oxides type catalyst and preparation method thereof of catalysis burning VOCs |
| CN110104667A (en) * | 2019-05-16 | 2019-08-09 | 福州大学 | A kind of magnalium hydrotalcite and preparation method and application for organic sulfur catalysis |
| CN110898783A (en) * | 2019-11-15 | 2020-03-24 | 江苏隆昌化工有限公司 | Preparation method of inorganic layered supramolecular material |
| CN111453750A (en) * | 2020-05-29 | 2020-07-28 | 山东长泽新材料科技有限公司 | Clean synthesis process of magnesium aluminum hydrotalcite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219248A (en) * | 2011-04-13 | 2011-10-19 | 东北大学 | Method for preparing hydrotalcite by adopting brucite |
| CN105271343A (en) * | 2015-10-21 | 2016-01-27 | 中电投山西铝业有限公司 | Production method of hydrocalumite |
| CN106745118A (en) * | 2016-12-30 | 2017-05-31 | 洛阳中超新材料股份有限公司 | A kind of magnalium hydrotalcite and the method for preparing magnalium hydrotalcite |
-
2017
- 2017-11-30 CN CN201711233019.0A patent/CN107902681B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219248A (en) * | 2011-04-13 | 2011-10-19 | 东北大学 | Method for preparing hydrotalcite by adopting brucite |
| CN105271343A (en) * | 2015-10-21 | 2016-01-27 | 中电投山西铝业有限公司 | Production method of hydrocalumite |
| CN106745118A (en) * | 2016-12-30 | 2017-05-31 | 洛阳中超新材料股份有限公司 | A kind of magnalium hydrotalcite and the method for preparing magnalium hydrotalcite |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052446A (en) * | 2018-10-19 | 2018-12-21 | 北京化工大学 | A method of calcium aluminium houghite is prepared using industrial residue for raw material |
| CN109437291A (en) * | 2018-12-24 | 2019-03-08 | 中南民族大学 | Hydrotalcite and preparation method thereof |
| CN109437291B (en) * | 2018-12-24 | 2021-01-26 | 中南民族大学 | Hydrotalcite and process for producing the same |
| CN109939683A (en) * | 2019-04-09 | 2019-06-28 | 江苏新沃催化剂有限公司 | A kind of ternary compound oxides type catalyst and preparation method thereof of catalysis burning VOCs |
| CN109939683B (en) * | 2019-04-09 | 2022-03-04 | 江苏新沃催化剂有限公司 | Ternary composite oxide type catalyst for catalytic combustion of VOCs and preparation method thereof |
| CN110104667A (en) * | 2019-05-16 | 2019-08-09 | 福州大学 | A kind of magnalium hydrotalcite and preparation method and application for organic sulfur catalysis |
| CN110104667B (en) * | 2019-05-16 | 2021-11-02 | 福州大学 | Magnesium-aluminum hydrotalcite for organic sulfur catalysis, and preparation method and application thereof |
| CN110898783A (en) * | 2019-11-15 | 2020-03-24 | 江苏隆昌化工有限公司 | Preparation method of inorganic layered supramolecular material |
| CN111453750A (en) * | 2020-05-29 | 2020-07-28 | 山东长泽新材料科技有限公司 | Clean synthesis process of magnesium aluminum hydrotalcite |
| CN111453750B (en) * | 2020-05-29 | 2021-09-03 | 山东长泽新材料科技有限公司 | Clean synthesis process of magnesium aluminum hydrotalcite |
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